【摘要】 查尔酮衍生化及其合成方法是合成工作者关注的一个热点。本文在微波辐射下,引入TBAB(四丁基溴化铵)作为相转移催化剂,以苯乙酮衍生物(1a~1d)、苯肼、苯乙酮衍生物(1e~1f)等为原料,合成了8种新的查尔酮衍生物(4a~4d,5a~5d);通过实验考察了物料比、微波辐射功率、微波辐射时间及催化剂用量等工艺条件对产物产率的影响;采用正交实验确定出查尔酮的最佳合成条件为:1,3-2苯基-4-甲酰基吡唑与苯乙酮物质的量比1∶1,微波输出功率为140 W,微波辐射间歇加热反应时间为30 min,四丁基溴化铵的量为0.4 g时,产率为87%~91%。更多还原

【Abstract】 4-formylpyrazole(3a~3d) were obtained by substituted acetophenones(1a~1d) and phenylhydrazine under microwave irradiation conditions.Eight chalcone derivative(4a ~4d,5a ~5d) were synthesized by 3a ~3d and substituted acetophenones in aqueous alkaline solution and TBAB(tertranutylammonium bromide)was phase transfer catalyst.The synthesis technology chalcone(4a) was studied.Effects of raw materials mole ratio,microwave radiation power,reaction time and dosage of phase transfer catalyst on the product yield were investigated.The optimum sythesis conditions are 1,3-2-phenyl-4-formylpyrazole to acetophenone mole ratio,microwave power reaction,microwave irradiation time,dosage of phase transfer catalyst are 1∶1,140 W,30 min and 0.4 g,respectively.The synthesis reaction were easily worked up with short time,high yields and green initiative.更多还原